ANALYTICAL AND BIOANALYTICAL CHEMISTRY
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2024
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IF 3.8
Li Chenjia,Liao Qi,Wang Rui,Zhang Xinping,Ma Mengyang,Liu Yonghong,Xiao Lei,Jiao Ying,Wang Nan
The scourge of drug addiction and abuse poses a significant challenge to society. Opioid drugs acting on μ-opioid receptor (OPRM1) make it one of the pivotal targets for drug addiction. In the past decade, sewage analysis has become a prevalent method of drug monitoring. However, traditional methods of detecting drugs in sewage are cumbersome, and rapid detection methods are relatively lacking. To address this, an innovative OPRM1-SNAP-tag/CMC method to directly identify drug components in sewage was established. Cell membrane chromatography (CMC) is an affinity chromatography technique which effectively detects receptor affinity substances. Cells constructed with high expression of specific receptor could be used to screen for compounds acting on the receptor. CMC based on OPRM1 provides a potentially convenient and effective tool for the detection of targeted drug components in sewage. In this study, the selectivity, reproducibility, column lifetime, and carryover of the CMC column had been assessed. Initially, we eluted the collected domestic sewage with methanol and acetonitrile, and the retention peaks were observed on the CMC system. Subsequently, without any preliminary sample preparation, we directly injected filtered samples of suspicious sewage into the OPRM1-SNAP-tag/CMC system, where we observed retention peaks as well. The retained components were further identified as morphine by using UPLC-MS/MS. In conclusion, the OPRM1-SNAP-tag/CMC method stands out as a reliable and robust model for the detection of drug components in sewage. It provides a valuable analytical tool for frontline drug control efforts, enhancing our capacity to monitor and mitigate the impact of drug abuse on society. Graphical Abstract
研究领域:
生物化学
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药物分析
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环境科学
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DOI
PubMed
高影响因子
CHEMICAL ENGINEERING JOURNAL
·
2025
·
IF 13.2
Shao-Lu Li,Qiyu Duan,Mengfan Wang,Bo Wu,Ning Yu,Genghao Gong,Yunxia Hu
In recent years, organic solvent nanofiltration (OSN) technology has garnered significant interest owing to its eco-friendly and low-carbon characteristics, offering efficient molecular separation in organic solvents. However, most scalable OSN membranes reported still suffer from the inherent permeability and selectivity trade-off effect, which inevitably hampers their industrial applications. In this study, we design and synthesize a novel bicyclic molecule 2,3,6,7-tetrahydroxy- maleimidoanthracene (THMIA), featuring a rigid, contorted configuration as well as four phenolic reactive groups. By exclusively employing THMIA reacted with trimesoyl chloride (TMC) through interfacial polymerization on a PAN substrate, we fabricate advanced TFC OSN membranes. The optimal THMIA/TMC composite membrane exhibits a high methanol permeance of 20.4 LMH/bar and good solutes retention ability with MWCO value as low as 289 Da. This outstanding separation performance should arise from the synergistic effects of crumpled membrane surface, elevated microporosity and ultra-thin thickness (∼14 nm) of the polyarylate nanofilm. In addition, the THMIA/TMC membrane shows promising prospects for the fast and reliable separation of various active pharmaceutical ingredients (APIs) and recovery of homogeneous organometallic catalyst from organic media. Overall, this study offers some new insights into utilization of the rigid bicyclic molecule as an aqueous IP monomer to facilely construct highly perm-selective OSN membranes.
研究领域:
材料科学
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化学工程
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环境科学
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产品关联
DOI
高影响因子
ACS Sustainable Chemistry & Engineering
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2024
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IF 7.1
Yong Song,Zhiyuan Jin,Jinsong Li,Wenjia Hao,Jiao Huang,Bo Jin,Rufang Peng
Although the mechanochemical synthesis of many active pharmaceutical ingredients (APIs) has been demonstrated, a technology that enables the large-scale continuous synthesis of thermosensitive APIs is lacking. In this work, we investigated the low-temperature continuous mechanochemical synthesis of a series of hydantoin-based derivatives, including the APIs nitrofurantoin and dantrolene, by using the previously proposed spiral gas–solid two-phase flow (S-GSF) technique. The structures of the prepared products were determined by using Fourier transform infrared spectroscopy, nuclear magnetic resonance, and powder X-ray diffractometry. Results showed that not a drop of organic solvent was used for the entire process, and high yields (not less than 94%) of E-isomer pure compounds were obtained without a complex purification step. Even with the low melting point of the raw material 5-nitrofurfural, nitrofurantoin could be synthesized continuously without remarkable amorphization. This situation distinguishes S-GSF from the existing mechanochemical methods. In addition, by improving system reactivity through cocrystallization and the highly efficient S-GSF technology, a continuous mechanochemical complete conversion of dantrolene was achieved for the first time, with a corresponding space-time yield up to 7.5 × 104 kg m–3 day–1. In particular, the crystalline form of dantrolene prepared in this way is a substable form dantr-V.
研究领域:
制药工程
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化学工程
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材料科学
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产品关联
DOI
高影响因子
JOURNAL OF COLLOID AND INTERFACE SCIENCE
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2024
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IF 9.4
Zhijie Yuan,Lingfeng Wang,Mengyuan Wu,Yuchao Niu,Yingshuang Meng,Xuehua Ruan,Gaohong He,Xiaobin Jiang
Active pharmaceutical ingredients (APIs) crystal preparation is a significant issue for the pharmaceutical development attributed to the effect on anti-inflammatory, anti-bacteria, and anti-viral, etc. While, the massive preparation of API crystal with high polymorphism selectivity is still a pendent challenge. Here, we firstly proposed a criterion according to the molecular aggregation, molecular orientation, and hydrogen bond energy between INA molecules from molecular dynamics (MD) simulations, which predicted the hydrogen bond architecture in crystal under different electric fields, hinting the recognition of crystal polymorphism. Then, an electric field governing confined liquid crystallization was constructed to achieve the INA crystal polymorphism screening relying on the criterion. Further, magnifying confined liquid volume by 5000 times from 1.0 μL to 5.0 mL realized the massive preparation of INA crystal with high polymorphic purity (>98.4%), giving a unique pathway for crystal engineering and pharmaceutical industry on the development of innovative and generic API based drugs.
研究领域:
药学
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材料科学
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计算化学
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产品关联
DOI
PubMed
高影响因子
ANALYTICAL CHEMISTRY
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2025
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IF 6.7
Huan Yao,Ting Huang,Zhifang Li,Huaxin Wu,Xueyao Li,Hua Tang,Fuhai Su,Xinliang Jin,Wei Zhang
Purity assessment is critical for the quality control of active pharmaceutical ingredients (APIs). However, there is a lack of rapid and accurate purity assessment methods that operate independently of target-specific certified reference materials (CRMs). Herein, we proposed a traceable quantification method, named SFC-ISC-qNMR, for purity assessment and quantitative determination of low-purity APIs, which was accomplished by tracing the test solution to the reference solution via supercritical fluid chromatography (SFC) collection with internal standard-correction (ISC), followed by an SI-traceable quantitative nuclear magnetic resonance (qNMR) analysis of the reference solution (SI = International System of Units). Digitoxin, a widely used cardiac glycoside in the treatment of heart failure and arrhythmias, was used as a model compound. By employing a mobile phase of supercritical CO2 modified with 24%–26% methanol, digitoxin with a purity exceeding 99.87% was isolated and collected. A national CRM of ethyl para-hydroxybenzoate was used as the IS for digitoxin. The SFC-ISC reference solution can be prepared in 15 min without the need for precise weighing, simply by reconstitution of the SFC collected high-purity analyte in deuterated methanol containing IS. The feasibility and reliability of the SFC-ISC-qNMR method were exhibited through the quantitative determination of digitoxin in chemical mixtures. The purity of a commercially available digitoxin reagent was determined to be 94.17% ± 0.15%, which was consistent with high-resolution qNMR analysis. The contents of spiked digitoxin in a digoxin analytical standard were measured at 1.06%, 1.37%, 2.39%, and 4.43%, respectively, showing high consistency with the gravimetric value with a bias less than 0.13%. In contrast, direct qNMR with deconvolution and HPLC analysis failed to provide accurate measurements. These results highlight the applicability of the SFC-ISC-qNMR method for drug evaluation and research, demonstrating its significant potential for the purity assessment of APIs.
研究领域:
分析化学
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药物分析
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色谱分析
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核磁共振（NMR）
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2017
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IF 3.255
Katerina Grigori,Yannis L. Loukas,Anđelija Malenović,Vicky Samara,Anastasia Kalaskani,Efi Dimovasili,Magda Kalovidouri,Yannis Dotsikas
A sensitive Liquid Chromatography tandem mass spectrometry (LC–MS/MS) method was developed and validated for the quantitative analysis of three potential genotoxic impurities (318BP, M9, S5) in meropenem Active Pharmaceutical Ingredient (API). Due to the requirement for LOD values in ppb range, a high concentration of meropenem API (30 mg/mL) had to be injected. Therefore, efficient determination of meropenem from its impurities became a critical aim of this study, in order to divert meropenem to waste, via a switching valve. After the selection of the important factors affecting analytes’ elution, a Box-Behnken design was utilized to set the plan of experiments conducted with UV detector. As responses, the separation factor s between the last eluting impurity and meropenem, as well as meropenem retention factor k were used. Grid point search methodology was implemented aiming to obtain the optimal conditions that simultaneously comply to the conflicted criteria. Optimal mobile phase consisted of ACN, methanol and 0.09% HCOOH at a ratio 71/3.5/15.5 v/v. All impurities and internal standard omeprazole were eluted before 7.5 min and at 8.0 min the eluents were directed to waste. The protocol was transferred to LC–MS/MS and validated according to ICH guidelines.
研究领域:
分析化学
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药物分析
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药学
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DOI
PubMed
高影响因子
MOLECULES
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2022
·Vol. 27
·期 13
·4129
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IF 4.927
Taiyu Wang,Hailong Yang,Jie Yang,Ningjie Guo,Guodong Wu,Xueyu Xu,Ming An
A novel method of ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) was developed for the identification and quantification of four potential genotoxic impurities (PGIs) in the active pharmaceutical ingredients of TSD-1, a novel P2Y12receptor antagonist. Four PGIs were named, 4-nitrobenzenesulfonic acid, methyl 4-nitrobenzenesulfonate, ethyl 4-nitrobenzenesulfonate, and isopropyl 4-nitrobenzenesulfonate. Following the International Conference of Harmonization (ICH) guidelines, this methodology is capable of quantifying four PGIs at 15.0 ppm in samples of 0.5 mg/mL concentration. This validated approach presented very low limits (0.1512–0.3897 ng/mL), excellent linearity (coefficients > 0.9900), and a satisfactory recovery range (94.9–115.5%). The method was sufficient in terms of sensitivity, linearity, precision, accuracy, selectivity, and robustness and, thus, has high practicality in the pharmaceutical quality control of TSD-1.Keywords:UPLC-MS/MS;genotoxic impurities;TSD-1;active pharmaceutical ingredients;quantitation;method validation
研究领域:
药物分析
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制药工程
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分析化学
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DOI
PubMed
高影响因子
LAB ON A CHIP
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2020
·Vol. 20
·期 11
·1907-1916
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IF 6.774
Zhenning Su,Jinxu He,Peipei Zhou,Lu Huang,Jianhua Zhou
Crystallization of active pharmaceutical ingredients (APIs) is a crucial process in the pharmaceutical industry due to its great impact in drug efficacy. However, conventional approaches for screening the optimal crystallization conditions of APIs are usually time-consuming, labor-intensive and expensive. Recently, droplet microfluidic technology has offered an alternative strategy for high-throughput screening of crystallization conditions. Despite its many advantages such as low sample consumption, reduced operation time, increased throughput, etc., some challenges remain to be solved, such as instability of droplets in the long-term and tedious efforts required for extracting useful information from massive data. To solve these problems, a high-throughput system that combined microfluidic hydrogel droplets with deep learning was proposed for the first time to screen the antisolvent-crystallization conditions of APIs. In this system, stable hydrogel droplets containing different concentrations of indomethacin, its solvent and antisolvent were generated on a chip. Crystals of indomethacin with different morphologies were formed in hydrogel droplets, and their optical images were captured by a camera. Then, deep learning was applied to identify the hundreds of indomethacin crystal images and successfully classify the crystal morphologies in a short time; a ternary phase diagram was drawn by combining the experimental results with the recognition results of crystal morphologies, and was used to guide the scale-up preparations of indomethacin crystals as desired. This system, which integrated high throughput preparation, characterization and data analysis, is also useful for screening the crystallization conditions and processes of semiconductors, catalysts, agrochemicals, proteins and other specialty chemicals.
研究领域:
药学
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化学工程
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材料科学
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数据科学
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产品关联
DOI
PubMed
高影响因子
FOOD RESEARCH INTERNATIONAL
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2023
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IF 8.1
Juan Wang,Danqing Wang,Mingquan Huang,Baoguo Sun,Fazheng Ren,Jihong Wu,Nan Meng,Jinglin Zhang
Huangjiu is a traditional Chinese alcoholic beverage, whose non-volatile chemical profile remains unclarified. Here, the non-volatile compounds of Huangjiu were first identified using a widely targeted metabolomics analysis. In total, 1146 compounds were identified, 997 of them were identified in Huangjiu for the first time. Moreover, 113 compounds were identified as key active ingredients of traditional Chinese medicines and 78 components were found as active pharmaceutical ingredients against 389 diseases. In addition, the comparative analysis and Kyoto Encyclopedia of Genes and Genomes pathway enrichment analysis revealed that Huangjiu from different regions differ in metabolite composition. Cofactor and amino acid biosynthesis and ABC transport were the dominant metabolic pathways. Furthermore, 7 metabolic pathways and 77 metabolic pathway regulatory markers were further found to be related with the different characteristics of different Huangjius. This study provides a theoretical and material basis for the quality control, health efficacy, and industrial development of Huangjiu.
研究领域:
食品科学
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代谢组学
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药理学
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中医药
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产品关联
DOI
PubMed
高影响因子
CHEMICAL ENGINEERING JOURNAL
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2021
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IF 13.273
Jinxu He,Jianhua Zhou,Jianpei Dong,Zhenning Su,Lu Huang
In the pharmaceutical industry, high-throughput crystallization (HTC) is an emerging strategy to accelerate the discovery of active pharmaceutical ingredients (APIs) with appropriate crystallization properties. It is typically processed in 96- and 384-well plates, which offer parallel crystallization vessels with microliter-scaled volume. However, the microwell size effect on crystallization kinetics at the scale of microtiters has not been fully investigated and remains unsolved. To address the issue, we proposed a novel deep-learning-based approach to investigate the effects of microwell sizes on the crystal growth kinetics of APIs. With a combination of microscopic imaging and deep learning, the massive information of indomethacin crystals was successfully obtained and analyzed in a high-throughput manner. And the relationships between crystallization properties (the average size, crystal size distribution, and the growth rate of crystals) and the size of the crystallization vessels were successfully revealed, which were further validated by the crystallization of ibuprofen and the scale-up experiment. Our research demonstrated the powerful capability of deep learning in processing complicated crystalline images. Moreover, our findings in the relationships between the size of the crystallization vessels and crystal growth kinetics are of great value in guiding the manufacture of APIs in the pharmaceutical industry.
研究领域:
药学
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材料科学
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化学工程
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人工智能
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产品关联
DOI
高影响因子
SCIENCE OF THE TOTAL ENVIRONMENT
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2022
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IF 10.753
Sathish Sundararaman,J. Aravind Kumar,Prabu Deivasigamani,Yuvarajan Devarajan
Water is one of the important gifts to mankind. In recent days the accessibility of pharmaceuticals in the environment is progressively a worldwide concern. The significant wellspring of these contaminations in water assets is drugs for human use or veterinary medications. Intermediates, active metabolites and raw materials present in water from pharmaceutical industry waste because of incomplete sewage treatment systems . Various pharmaceutical components such as analgesic/antipyretics such as Ibuprofen (57.9–104 ng/L), Diclofenac (17–129 ng/L), antibiotics such as Sulfamethoxazole (28.7–124.5 ng/L), Sulfamethazine (29.2–83.9 ng/L), Azithromycin (10–68 ng/L), psychiatric drug such as Carbamazepine (9.3–92.4 ng/L), stimulants such as caffeine greater than 55 ng/L, antidepressants, antihypertensive, contraceptives etc., are present in water resources and have been detected in mg/L to μg/L range. The synergic effects and ecotoxicological hazard assessment must be developed. Studies demonstrate that these drugs might cause morphological, metabolic and sex alterations on sea-going species, and interruption of biodegradation activities. Hazard analysis and assessments are in progress. However, the conventional effluent treatment methods are not sufficient to remove API (active pharmaceutical ingredients) from this water effectively. There is necessitate for continuous monitoring of the pharmaceutical compounds in aquatic ecosystem to save the environment and living form of lives from health hazards. This work highlights the hazards, environmental assessment and the mitigation measures of pharmaceutical pollutants.
研究领域:
环境科学
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水资源管理
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毒理学
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药学
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生态学
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DOI
PubMed
高影响因子
JOURNAL OF MOLECULAR STRUCTURE
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2025
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IF 4.7
Fumin Xue,Xinyue Yuan,Fengying Wu,Jingling Liu,Yan Cheng
L -Abrine (N-Methyl- L -tryptophan, L-ABR) shows antioxidant and radical scavenging abilities in vitro but has low solubility. This research introduces a new L -abrine-oxalate (L-ABR-OXA) salt using grinding and solvent evaporation techniques. The structure was confirmed by single-crystal X-ray diffraction (SXRD), and its purity and stability were validated through PXRD, TGA, DSC, and FTIR analyses. A key innovation is the significant increase in solubility of L-ABR (4 times in water and 3 times in PBS) achieved through oxalate salt formation. This enhancement is backed by molecular electrostatic potential (MEP) and Hirshfeld surface analysis, which proved that hydrogen bonds are the primary factor driving the formation of salts. Antioxidant tests showed that L-ABR-OXA has superior radical scavenging and antioxidant activity at low concentrations compared to pure L-ABR, indicating its potential as a more effective bioactive formulation. This study offers a crystallography-based approach to improve the solubility and bioactivity of poorly soluble active pharmaceutical ingredients (API).
研究领域:
药物化学
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晶体工程
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药物递送
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抗氧化研究
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材料科学
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物理化学
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产品关联
DOI
高影响因子
危险品化学品经营许可证（带存储）